阅读说明：本技术 一种氨肟化兼回收叔丁醇的反应系统及方法 (Reaction system and method for ammoximation and recovery of tert-butyl alcohol ) 是由 张志炳 周政 张锋 李磊 孟为民 王宝荣 杨高东 罗华勋 杨国强 田洪舟 曹宇 于 2020-04-13 设计创作，主要内容包括：本发明提供了一种氨肟化兼回收叔丁醇的反应系统及方法,包括肟化反应器、反应清液缓冲罐、尾气吸收塔、叔丁醇回收塔和叔丁醇回流罐,其中,肟化反应器的顶部设置有尾气出口,肟化反应器的底部设置有出料口,出料口与所述反应清液缓冲罐连接,尾气出口与所述尾气吸收塔连接,反应清液缓冲罐出来的物料从叔丁醇回收塔的中段通入,叔丁醇回收塔的顶部与叔丁醇回流罐连接,肟化反应器外部设置有外循环换热装置,内部设置有微界面发生器,用于分散破碎气体。本发明的氨肟化兼回收叔丁醇的反应系统,通过在反应器内部设置了微界面发生器后,增大了气液相的传质面积,降低了反应温度和压力,从而抑制了副反应的发生,提高了肟化反应效率。(The invention provides a reaction system and a method for ammoximation and recovery of tert-butyl alcohol, which comprises an oximation reactor, a reaction clear liquid buffer tank, a tail gas absorption tower, a tert-butyl alcohol recovery tower and a tert-butyl alcohol reflux tank, wherein the top of the oximation reactor is provided with a tail gas outlet, the bottom of the oximation reactor is provided with a discharge port, the discharge port is connected with the reaction clear liquid buffer tank, the tail gas outlet is connected with the tail gas absorption tower, materials discharged from the reaction clear liquid buffer tank are introduced from the middle section of the tert-butyl alcohol recovery tower, the top of the tert-butyl alcohol recovery tower is connected with the tert-butyl alcohol reflux tank, an external circulation heat exchange device is arranged outside the oximation reactor, and a micro-interface generator is arranged inside the oximation reactor and used for. According to the reaction system for ammoximation and recovery of tert-butyl alcohol, the micro-interface generator is arranged in the reactor, so that the mass transfer area of a gas-liquid phase is increased, and the reaction temperature and pressure are reduced, so that the side reaction is inhibited, and the oximation reaction efficiency is improved.)

1. A reaction system for ammoximation and recovery of tert-butyl alcohol is characterized by comprising an oximation reactor, a reaction clear liquid buffer tank, a tail gas absorption tower, a tert-butyl alcohol recovery tower and a tert-butyl alcohol reflux tank, wherein,

a tail gas outlet is formed in the top of the oximation reactor, a discharge hole is formed in the bottom of the oximation reactor, the discharge hole is connected with the reaction clear liquid buffer tank, the tail gas outlet is connected with the tail gas absorption tower, materials from the reaction clear liquid buffer tank are introduced from the middle section of the tert-butyl alcohol recovery tower to be used for recovering tert-butyl alcohol, and the top of the tert-butyl alcohol recovery tower is connected with the tert-butyl alcohol reflux tank to be used for gas-liquid separation;

an external circulation heat exchange device is arranged outside the oximation reactor and is used for controlling the temperature inside the oximation reactor; the interior of the oximation reactor is provided with a micro-interface generator which is used for dispersing the broken gas into micro-bubbles with the diameter of micron level.

2. The reaction system for ammoximation and recovery of tert-butanol according to claim 1, wherein the side wall of the oximation reactor is provided with an air inlet for introducing raw ammonia gas, the air inlet extends to the inside of the micro-interface generator through a pipeline, the type of the micro-interface generator is a pneumatic micro-interface generator, the number of the micro-interface generators is more than one, and each micro-interface generator is connected in parallel.

3. The reaction system for ammoximation and recovery of tert-butanol according to claim 1, wherein a liquid inlet and a gas inlet are respectively arranged at the middle section of the tert-butanol recovery tower, and the liquid inlet is connected with the bottom of the reaction clear liquid buffer tank; the gas inlet is connected with the top of the reaction clear liquid buffer tank.

4. The reaction system for ammoximation and recovery of tertiary butanol according to claim 1, wherein the top of the tertiary butanol recovery tower is provided with an overhead condenser, and the bottom of the tower is provided with a bottom reboiler.

5. The reaction system for ammoximation and recovery of tert-butanol according to claim 1, further comprising a return line, wherein one end of the return line is connected with the top of the tert-butanol recovery column, and the other end of the return line is connected with the bottom of the tert-butanol return tank for returning the substances in the tert-butanol return tank to continue separation and purification; and a reflux pump is arranged on the reflux pipeline.

6. The reaction system for ammoximation and recovery of tert-butanol according to claim 1, wherein a pipeline connecting the tail gas outlet and the tail gas absorption tower is provided with an exhaust gas cooler, the tert-butanol reflux tank is provided with a non-condensable gas outlet, and the non-condensable gas outlet is connected with the exhaust gas cooler so that the non-condensable gas and the tail gas are mixed and then enter the tail gas absorption tower for recycling.

7. The ammoximation and tertiary butanol recovery reaction system of any one of claims 1-6, wherein the tertiary butanol recovery column is of the type of a vertical sieve plate column.

8. The ammoximation and tert-butanol recovery reaction system according to any one of claims 1 to 6, wherein the reaction system further comprises a circulating tert-butanol tank, the top of the circulating tert-butanol tank is connected with the bottom of the tert-butanol reflux tank, and the bottom of the circulating tert-butanol tank is connected with the bottom of the oximation reactor, so that tert-butanol can be reused as a reaction solvent.

9. The method for ammoximation and recovery of tert-butanol using the reaction system for ammoximation and recovery of tert-butanol according to any one of claims 1 to 8, comprising the steps of:

after ammonia gas is dispersed and crushed into micro bubbles, the micro bubbles and liquid-phase materials are subjected to catalytic oximation reaction; in the process of carrying out the catalytic oximation reaction, the gas which is not completely reacted is recycled, and the tertiary butanol in the reaction product is recycled after the reaction product is collected in a clear liquid manner.

10. The process of claim 9, wherein the temperature of the oximation reaction is 80-82 ℃ and the pressure is 0.18-0.23 MPa.

Technical Field

The invention belongs to the technical field of intensified reactions, and particularly relates to a reaction system and a method for ammoximation and recovery of tert-butyl alcohol.

Background

Caprolactam is an important organic compound, and downstream products of caprolactam are widely applied to the industries of spinning, tires, food packaging and the like. The production process mostly adopts ammoximation to produce cyclohexanone oxime, and then liquid phase rearrangement is carried out to produce caprolactam, and the ammoximation reaction of the cyclohexanone is a core control program in the process. In the cyclohexanone ammoximation reaction process, factors influencing the reaction mainly comprise mass transfer efficiency, reaction temperature and pressure, reaction time, catalyst concentration and raw material ratio and the like, and researches show that the mass transfer efficiency and the reaction temperature and pressure have great influence on production; on the other hand, the oximation reaction is a strong exothermic reaction, the temperature and the pressure are too high, the decomposition products of cyclohexanone and cyclohexanone oxime are increased, and the products are not easy to remove in the post-process, and the yield and the quality of the final product caprolactam are influenced.

In conclusion, in order to improve the efficiency of the oximation reaction, reduce the reaction temperature and pressure and reduce the occurrence of side reactions, the improvement of the ammoximation industrialization device is a problem which needs to be solved urgently to reduce the ammoximation cost and improve the ammoximation production load.

Disclosure of Invention

In view of the above, the first objective of the present invention is to provide a reaction system for ammoximation and recovery of tert-butanol, the reaction system is provided with a micro-interface generator inside the ammoximation reactor, and after the micro-interface generator is provided, on one hand, ammonia gas can be dispersed and crushed into micro-bubbles with micron-sized diameters, and the phase interface area between ammonia gas and liquid phase materials is increased, so that the mass transfer space is fully satisfied, the residence time of ammonia gas in the liquid phase is increased, and the consumption of ammonia gas is reduced, thereby greatly improving the efficiency of the ammoximation reaction, effectively inhibiting side reactions, and significantly reducing the energy consumption in the reaction process; on the other hand, the reaction temperature and pressure are reduced, the decomposition products of cyclohexanone and cyclohexanone oxime are reduced, the yield and quality of the final product caprolactam are improved, the energy consumption is reduced, and the system safety is improved.

The second purpose of the invention is to provide a method for carrying out reaction by adopting the reaction system, the method has mild operation conditions, reduces the temperature and pressure of oximation reaction while ensuring the reaction efficiency, has high safety performance and low energy consumption, and achieves better reaction effect than the prior art.

In order to achieve the above purpose of the present invention, the following technical solutions are adopted:

the invention provides a reaction system for ammoximation and recovery of tertiary butanol, which is characterized by comprising an oximation reactor, a reaction clear liquid buffer tank, a tail gas absorption tower, a tertiary butanol recovery tower and a tertiary butanol reflux tank, wherein,

a tail gas outlet is formed in the top of the oximation reactor, a discharge hole is formed in the bottom of the oximation reactor, the discharge hole is connected with the reaction clear liquid buffer tank, the tail gas outlet is connected with the tail gas absorption tower, materials from the reaction clear liquid buffer tank are introduced from the middle section of the tert-butyl alcohol recovery tower to be used for recovering tert-butyl alcohol, and the top of the tert-butyl alcohol recovery tower is connected with the tert-butyl alcohol reflux tank to be used for gas-liquid separation;

an external circulation heat exchange device is arranged outside the oximation reactor and is used for controlling the temperature inside the oximation reactor; the interior of the oximation reactor is provided with a micro-interface generator which is used for dispersing the broken gas into micro-bubbles with the diameter of micron level.

Drawings

Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:

FIG. 1 is a schematic structural diagram of a reaction system for ammoximation and recovery of tert-butanol according to an embodiment of the present invention.

Detailed Description

The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.

In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.

In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.